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WO2018139563A1 - POUDRE MAGNÉTIQUE À AIMANTATION PROVISOIRE, POUDRE D'ALLIAGE NANOCRISTALLIN À BASE DE Fe, COMPOSANT MAGNÉTIQUE ET NOYAU DE POUSSIÈRE - Google Patents

POUDRE MAGNÉTIQUE À AIMANTATION PROVISOIRE, POUDRE D'ALLIAGE NANOCRISTALLIN À BASE DE Fe, COMPOSANT MAGNÉTIQUE ET NOYAU DE POUSSIÈRE Download PDF

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Publication number
WO2018139563A1
WO2018139563A1 PCT/JP2018/002380 JP2018002380W WO2018139563A1 WO 2018139563 A1 WO2018139563 A1 WO 2018139563A1 JP 2018002380 W JP2018002380 W JP 2018002380W WO 2018139563 A1 WO2018139563 A1 WO 2018139563A1
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WIPO (PCT)
Prior art keywords
soft magnetic
magnetic powder
less
powder
mass
Prior art date
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Ceased
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PCT/JP2018/002380
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English (en)
Japanese (ja)
Inventor
浦田　顕理
美帆 千葉
村木　峰男
誠 中世古
拓也 高下
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JFE Steel Corp
Tokin Corp
Original Assignee
JFE Steel Corp
Tokin Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JFE Steel Corp, Tokin Corp filed Critical JFE Steel Corp
Priority to US16/481,449 priority Critical patent/US11814707B2/en
Priority to SE1950904A priority patent/SE543592C2/en
Priority to CA3051184A priority patent/CA3051184C/fr
Priority to JP2018552901A priority patent/JP6472939B2/ja
Priority to CN201880008431.9A priority patent/CN110225801B/zh
Priority to KR1020197021757A priority patent/KR102259446B1/ko
Publication of WO2018139563A1 publication Critical patent/WO2018139563A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/08—Metallic powder characterised by particles having an amorphous microstructure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/002—Making metallic powder or suspensions thereof amorphous or microcrystalline
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/02—Amorphous alloys with iron as the major constituent
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/153—Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15333—Amorphous metallic alloys, e.g. glassy metals containing nanocrystallites, e.g. obtained by annealing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/35—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2200/00—Crystalline structure
    • C22C2200/02—Amorphous
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2200/00—Crystalline structure
    • C22C2200/04—Nanocrystalline
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C2202/00—Physical properties
    • C22C2202/02—Magnetic
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60

Definitions

  • the present invention relates to a soft magnetic powder suitable for use in magnetic parts such as a transformer, an inductor, and a magnetic core of a motor.
  • Patent Document 1 This type of soft magnetic powder is disclosed in Patent Document 1, for example.
  • Patent Document 1 discloses an alloy composition composed of Fe, B, Si, P, C, and Cu.
  • the alloy composition of Patent Document 1 has a continuous ribbon shape or a powder shape.
  • a powder-shaped alloy composition (soft magnetic powder) is produced, for example, by an atomizing method, and has an amorphous phase (amorphous phase) as a main phase.
  • the soft magnetic powder is subjected to heat treatment under predetermined heat treatment conditions to precipitate bccFe nanocrystals, thereby obtaining an Fe-based nanocrystalline alloy powder.
  • a magnetic component having excellent magnetic properties can be obtained.
  • soft magnetic powder When obtaining Fe-based nanocrystalline alloy powder from soft magnetic powder, from the viewpoint of obtaining Fe-based nanocrystalline alloy powder having sufficient magnetic properties, soft magnetic powder is substantially only from an amorphous phase (amorphous phase). (That is, the crystallinity is extremely low).
  • amorphous phase amorphous phase
  • expensive raw materials are required, and complicated processes such as excluding large-diameter powders by classification after atomization are required. That is, the manufacturing cost increases.
  • an object of the present invention is to provide a soft magnetic powder capable of producing an Fe-based nanocrystalline alloy powder having sufficient magnetic properties while avoiding an increase in manufacturing cost.
  • a predetermined composition range suitable for soft magnetic powder was obtained while not suitable for a continuous ribbon.
  • This composition range is not suitable for forming a continuous ribbon because the required uniformity cannot be obtained due to the mixture of crystals.
  • an Fe-based nanocrystalline alloy powder having sufficient magnetic properties was obtained by suppressing the crystallinity before heat treatment to 10% or less. Specifically, even if it is a soft magnetic powder containing a certain amount of crystallites (crystalline phase), if the crystallinity is 10% or less, the Fe-based nanocrystalline alloy powder after heat treatment has a crystallinity of extremely zero. The magnetic properties were almost inferior to those of the Fe-based nanocrystalline alloy powder obtained from the near soft magnetic powder.
  • the present invention provides the following soft magnetic powder having this composition range.
  • One aspect of the present invention is a soft magnetic powder represented by the composition formula Fe a Si b B c P d Cu e excluding inevitable impurities, wherein 79 ⁇ a ⁇ 84.5 at%, 0 ⁇ b ⁇ 6 at%.
  • the soft magnetic powder according to the present invention contains Fe, Si, B, P and Cu in a predetermined range, the crystallinity can be suppressed to 10% or less.
  • an Fe-based nanocrystalline alloy powder having sufficient magnetic properties can be obtained by a heat treatment similar to the conventional one.
  • the Fe-based nanocrystalline alloy powder having sufficient magnetic properties can be produced while avoiding an increase in manufacturing cost by allowing a certain degree of crystallinity of 10% or less rather than making the crystallinity very close to zero.
  • Soft magnetic powder can be obtained.
  • the soft magnetic powder according to the present embodiment is represented by the composition formula Fe a Si b B c P d Cu e except for inevitable impurities.
  • the soft magnetic powder according to the embodiment of the present invention can be used as a starting material for Fe-based nanocrystalline alloy powder.
  • the Fe-based nanocrystalline alloy powder produced from the soft magnetic powder of the present embodiment can be used as a material for producing various magnetic parts and dust cores.
  • the soft magnetic powder of the present embodiment can be used as a direct material for producing various magnetic parts and dust cores.
  • the soft magnetic powder of the present embodiment can be manufactured by a manufacturing method such as an atomizing method.
  • the soft magnetic powder thus produced has an amorphous phase (amorphous phase) as the main phase.
  • amorphous phase amorphous phase
  • bccFe ( ⁇ Fe) nanocrystals are precipitated, thereby obtaining an Fe-based nanocrystalline alloy powder having excellent magnetic properties. That is, the Fe-based nanocrystalline alloy powder of the present embodiment is an Fe-based alloy containing an amorphous phase as a main phase and containing bccFe nanocrystals.
  • ⁇ Fe microcrystals initial precipitates
  • the initial precipitate contributes to the deterioration of the magnetic properties of the Fe-based nanocrystalline alloy powder.
  • nanocrystals having a particle size exceeding 50 nm may precipitate in the Fe-based nanocrystalline alloy powder.
  • Nanocrystals having a particle size exceeding 50 nm inhibit the movement of the domain wall only by being deposited in a small amount, and deteriorate the magnetic properties of the Fe-based nanocrystalline alloy powder.
  • the initial crystallinity (hereinafter simply referred to as “crystallinity”), which is the volume ratio of the initial precipitate to the soft magnetic powder, is made as low as possible to be substantially amorphous. It is considered desirable to produce a soft magnetic powder consisting only of phases. However, to obtain a soft magnetic powder with a very low degree of crystallinity, expensive raw materials are required, and complicated processes such as excluding large-diameter powders by classification after atomization are required. That is, the manufacturing cost increases.
  • the soft magnetic powder of the composition formula Fe a Si b B c P d Cu e is Fe of 79 at% or more and 84.5 at% or less, Si of less than 6 at% (including zero). 4 at% or more and 10 at% or less of B, 4 at% or more and 11 at% or less of P, and 0.2 at% or more and less than 0.4 at% of Cu are included.
  • This composition range (hereinafter referred to as “predetermined range”) is not suitable for forming a continuous ribbon because the required uniformity cannot be obtained due to the mixture of crystals (initial precipitates).
  • the crystallinity may be about 10%.
  • the continuous ribbon may be partially weakened due to the initial precipitate. Furthermore, even after nanocrystallization, a uniform fine structure cannot be obtained, and the magnetic properties may be significantly deteriorated.
  • the problems described above are inherent to continuous ribbons.
  • the soft magnetic powder structural problems hardly occur even when the crystallinity is about 10%. Furthermore, if the crystallinity can be suppressed to 10% or less, the pinning sites of the domain wall are reduced. Specifically, when the crystallinity is suppressed to 10% or less, precipitation of nanocrystals having a particle size exceeding 50 nm in the Fe-based nanocrystalline alloy powder can be suppressed even by the same heat treatment as before, and the crystallinity becomes extremely zero. An Fe-based nanocrystalline alloy powder having sufficient magnetic properties that is almost inferior to that of an Fe-based nanocrystalline alloy powder obtained from a near soft magnetic powder can be obtained.
  • the soft magnetic powder according to the present embodiment contains Fe, Si, B, P and Cu in a predetermined range, the crystallinity can be suppressed to 10% or less.
  • an Fe-based nanocrystalline alloy powder having sufficient magnetic properties can be obtained by a heat treatment similar to the conventional one.
  • the Fe-based nanocrystalline alloy powder having sufficient magnetic properties can be produced while avoiding an increase in manufacturing cost by allowing a certain degree of crystallinity of 10% or less rather than making the crystallinity very close to zero.
  • Soft magnetic powder can be obtained. More specifically, according to the present embodiment, soft magnetic powder can be stably produced from a relatively inexpensive raw material using a general atomizing apparatus. Moreover, production conditions such as the melting temperature of the raw material can be relaxed.
  • a soft magnetic powder having an amorphous phase as a main phase and containing ⁇ Fe microcrystals (crystalline phase due to initial precipitates) in a volume ratio of 10% or less is provided.
  • the soft magnetic powder may contain a crystal phase of 3% or less by volume. In order to make the crystallinity 3% or less, it is preferable that a ⁇ 83.5 at%, c ⁇ 8.5 at%, and d ⁇ 5.5 at%.
  • the degree of crystallinity is 3% or less
  • the molding density when a dust core is produced is improved. Specifically, when the crystallinity exceeds 3%, the molding density may be reduced. However, when the crystallinity is 3% or less, a reduction in the molding density can be suppressed, and thus the magnetic permeability can be maintained.
  • the crystallinity is 3% or less, it is easy to maintain the appearance of the soft magnetic powder. Specifically, if the crystallinity exceeds 3%, the atomized soft magnetic powder may be discolored by oxidation, but if the crystallinity is 3% or less, discoloration of the soft magnetic powder is suppressed and the appearance is reduced. Can be maintained.
  • the soft magnetic powder according to the present embodiment When the soft magnetic powder according to the present embodiment is heat-treated in an inert atmosphere such as an Ar gas atmosphere, crystallization can be confirmed twice or more.
  • the temperature at which crystallization starts first is called the first crystallization start temperature (T x1 ), and the temperature at which the second crystallization starts is called the second crystallization start temperature (T x2 ).
  • the first crystallization start temperature (T x1 ) is an exothermic peak of nanocrystal precipitation of bccFe
  • the second crystallization start temperature (T x2 ) is an exothermic peak of precipitation of compounds such as FeB and FeP.
  • These crystallization temperatures can be evaluated by performing thermal analysis at a rate of temperature increase of about 40 ° C./min using, for example, a differential scanning calorimetry (DSC) apparatus.
  • DSC differential scanning calorimetry
  • composition range of the soft magnetic powder according to the present embodiment will be described in more detail.
  • the Fe element is a main element and an essential element responsible for magnetism.
  • the ratio of Fe is large.
  • the proportion of Fe according to the present embodiment is 79 at% or more and 84.5 at% or less.
  • the Fe ratio needs to be 79 at% or more in order to obtain a desired saturation magnetic flux density Bs in the Fe-based nanocrystalline alloy powder, and in order to produce a soft magnetic powder having a crystallinity of 10% or less. 84.5 at% or less.
  • the ratio of Fe is more preferably 80 at% or more in order to improve the saturation magnetic flux density Bs.
  • the proportion of Fe is preferably 83.5 at% or less in order to reduce the core loss of the dust core by setting the crystallinity to 3% or less.
  • the Si element is an element responsible for forming an amorphous phase, and contributes to the stabilization of the nanocrystal in the nanocrystallization.
  • the Si ratio needs to be less than 6 at% (including zero).
  • the Si ratio is preferably 2 at% or more in order to improve the saturation magnetic flux density Bs of the Fe-based nanocrystalline alloy powder, and more preferably 3 at% or more in order to increase ⁇ T.
  • the B element is an essential element responsible for forming an amorphous phase.
  • the ratio of B needs to be 4 at% or more and 10 at% or less in order to reduce the core loss of the dust core by suppressing the crystallinity of the soft magnetic powder to 10% or less. Further, the ratio of B is preferably 8.5 at% or less in order to further reduce the core loss of the dust core by suppressing the crystallinity of the soft magnetic powder to 3% or less.
  • the P element is an essential element for forming an amorphous phase.
  • the proportion of P according to the present embodiment is greater than 4 at% and less than or equal to 11 at%.
  • the spherical soft magnetic powder is preferable from the viewpoint of reducing the viscosity of the molten alloy when producing the soft magnetic powder and improving the magnetic properties of the dust core. It becomes easy to produce.
  • the melting point is lowered, the amorphous forming ability can be improved, and the Fe-based nanocrystalline alloy powder can be easily produced.
  • the proportion of P needs to be 11 at% or less in order to obtain a desired saturation magnetic flux density Bs in the Fe-based nanocrystalline alloy powder.
  • the ratio of P is preferably larger than 5.0 at% in order to improve corrosion resistance, more preferably 5.5 at% or more in order to make the crystallinity 3% or less, and Fe group nano In order to reduce the core loss of the dust core by refining the nanocrystals in the crystal alloy powder, it is more preferably 6 at% or more.
  • the ratio of P is preferably 10 at% or less and more preferably 8 at% or less in order to improve the saturation magnetic flux density Bs.
  • Cu element is an essential element contributing to nanocrystallization.
  • the proportion of Cu according to the present embodiment is 0.2 at% or more and less than 0.4 at%.
  • the Cu ratio needs to be 0.2 at% or more in order to prevent nanocrystal coarsening in the Fe-based nanocrystalline alloy powder and obtain a desired core loss in the dust core, In order to suppress the crystallinity to 10% or less by the crystal forming ability, it is necessary to make it less than 0.4 at%.
  • the Cu ratio is preferably 0.3 at% or more in order to refine the nanocrystals in the Fe-based nanocrystalline alloy powder and reduce the core loss of the dust core, thereby increasing the precipitation amount of the nanocrystals.
  • it is more preferably 0.35 at% or more.
  • the soft magnetic powder according to the present embodiment may contain inevitable impurities such as Al, Ti, S, O, and N contained in the raw material in addition to Fe, P, Cu, Si, and B.
  • these inevitable impurities tend to promote crystallization by forming crystal grains of ⁇ Fe microcrystals (initial precipitates) in the soft magnetic powder.
  • the ratio (content) of these inevitable impurities in the soft magnetic powder is large, the degree of crystallinity tends to be high, and the variation in the grain size of the ⁇ Fe microcrystals tends to be large. Therefore, the content of inevitable impurities in the soft magnetic powder is preferably as small as possible.
  • the content of the main component elements (Fe, P, Cu, Si and B) of the soft magnetic powder is indicated by at%.
  • an element added to the main component element to improve the characteristics of the soft magnetic powder for example, Cr that improves the corrosion resistance of the soft magnetic powder, Nb that improves the amorphous property of the soft magnetic powder,
  • the content of an element such as Mo is indicated by at%.
  • the content of the impurity element which adversely affects the characteristics of the soft magnetic powder and wants to be reduced as much as possible, but which is mixed in consideration of the manufacturing process, raw material price, etc. is indicated by mass% (mass%).
  • Al is a trace element mixed in soft magnetic powder by using industrial raw materials such as Fe—P and Fe—B.
  • the proportion of the amorphous phase in the soft magnetic powder is lowered and the soft magnetic characteristics are lowered.
  • the content of Al is preferably 0.1% by mass or less in order to suppress a decrease in the proportion of the amorphous phase.
  • the Al content is more preferably 0.01% by mass or less in order to suppress a decrease in the proportion of the amorphous phase and suppress a decrease in soft magnetic properties.
  • Ti is a trace element mixed in the soft magnetic powder by using industrial raw materials such as Fe-P and Fe-B.
  • the Ti content is preferably 0.1% by mass or less in order to suppress a decrease in the proportion of the amorphous phase.
  • the Ti content is more preferably 0.01% by mass or less in order to suppress a decrease in the proportion of the amorphous phase and to suppress a decrease in soft magnetic properties.
  • S is a trace element mixed in the soft magnetic powder by using industrial raw materials such as Fe—P and Fe—B.
  • industrial raw materials such as Fe—P and Fe—B.
  • S By adding S in a small amount to the soft magnetic powder, it becomes easy to produce a spherical soft magnetic powder.
  • the S content is preferably 0.1% by mass or less, and more preferably 0.05% by mass or less, in order to suppress a decrease in soft magnetic properties.
  • O is a trace element that is mixed into the soft magnetic powder by using industrial raw materials, and is mixed into the soft magnetic powder from the air or water during atomization and drying.
  • water atomization it is known that the O content tends to increase because the surface area of the powder increases as the particle size of the powder decreases.
  • the content of O is preferably 1.0% by mass or less in order to suppress a decrease in the proportion of the amorphous phase.
  • the O content is more preferably 0.3% by mass or less in order to suppress a decrease in filling rate when molding the soft magnetic powder and to suppress a decrease in soft magnetic properties.
  • N is a trace element that is mixed in the soft magnetic powder by using industrial raw materials and mixed in the soft magnetic powder from the air during heat treatment.
  • the N content is preferably 0.01% by mass or less, and preferably 0.002% by mass or less in order to suppress a decrease in the proportion of the amorphous phase and to suppress a decrease in soft magnetic properties. More preferably it is.
  • the composition formula of the soft magnetic powder excluding inevitable impurities is Fe a Si b B c P d Cu e . Therefore, the composition formula of soft magnetic powder including inevitable impurities composed of Al, Ti, S, O and N among the inevitable impurities is (Fe a Si b B c P d Cu e ) 100- ⁇ X ⁇ . .
  • X is an inevitable impurity composed of Al, Ti, S, O, and N
  • ⁇ is a ratio (mass%) of X contained in the soft magnetic powder.
  • the preferable range of a, b, c, d, e (at%) is as already described.
  • the soft magnetic powder contains one or more elements selected from Al, Ti, S, O, and N as inevitable impurities
  • the Al content is 0.1% by mass or less
  • the Ti content Is 0.1 mass% or less
  • S content is 0.1 mass% or less
  • O content is 1.0 mass% or less
  • N content is 0.01 mass% or less.
  • the value of ⁇ indicating the ratio of Al, Ti, S, O, N (inevitable impurities X) contained in the soft magnetic powder is preferably 1.31% by mass or less.
  • the soft magnetic powder contains one or more elements selected from Al, Ti, S, O, and N as inevitable impurities
  • the Al content is 0.01% by mass or less, and the Ti content Is 0.01 mass% or less, S content is 0.05 mass% or less, O content is 0.3 mass% or less, and N content is 0.002 mass% or less. More preferably it is. Therefore, in this case, the value of ⁇ indicating the ratio of Al, Ti, S, O, N (inevitable impurities X) contained in the soft magnetic powder is more preferably 0.372% by mass or less.
  • a part of Fe is mixed with Cr, V, Mn, Co, Ni, Zn, Nb, Zr, Hf, Mo, Ta, W, Ag, Au, Pd, K, Ca,
  • One or more elements selected from Mg, Sn, C, Y and rare earth elements may be substituted.
  • the atomic weight (substitution atomic weight) substituted for the above elements in Fe needs to be within a range that does not adversely affect the melting conditions such as magnetic properties, amorphous form performance, melting point, and raw material price.
  • the preferred substituted atomic weight is 3 at% or less of Fe
  • the further preferred substituted atomic weight is 1.5 at% or less of Fe.
  • M in these composition formulas is Cr, V, Mn, Co, Ni, Zn, Nb, Zr, Hf, Mo, Ta, W, Ag, Au, Pd, K, Ca, Mg, Sn, C, Y and One or more elements selected from rare earth elements.
  • the preferable range of a, b, c, d, e (at%) is as already described.
  • the soft magnetic powder, the Fe-based nanocrystalline alloy powder, the magnetic component, and the dust core in the present embodiment will be described in more detail while explaining the manufacturing method thereof.
  • the soft magnetic powder according to the present embodiment can be produced by various manufacturing methods.
  • the soft magnetic powder may be produced by an atomizing method such as a water atomizing method or a gas atomizing method.
  • the powder preparation process by the atomizing method first, raw materials are prepared. Next, the raw materials are weighed so as to have a predetermined composition and melted to produce a molten alloy. At this time, since the soft magnetic powder of the present embodiment has a low melting point, power consumption for dissolution can be reduced. Next, the molten alloy is discharged from the nozzle and divided into alloy droplets using high-pressure water or gas, thereby producing a fine soft magnetic powder.
  • the gas used for cutting may be an inert gas such as argon or nitrogen.
  • the alloy droplets immediately after the division may be brought into contact with a cooling liquid or solid to be rapidly cooled, or the alloy droplets may be redivided and further refined.
  • a liquid for cooling for example, water or oil may be used.
  • a solid for cooling, for example, a rotating copper roll or a rotating aluminum plate may be used.
  • the cooling liquid or solid is not limited to this, and various materials can be used.
  • the powder shape and particle size of the soft magnetic powder can be adjusted by changing the production conditions.
  • the viscosity of the molten alloy is low, it is easy to produce a soft magnetic powder into a spherical shape.
  • the average particle diameter of the soft magnetic powder is preferably 200 ⁇ m or less and more preferably 50 ⁇ m or less in order to reduce the crystallinity.
  • the maximum particle diameter of the soft magnetic powder is preferably 200 ⁇ m or less.
  • initial precipitates are precipitated in the soft magnetic powder having an amorphous phase as a main phase.
  • a compound such as FeB or FeP is precipitated as the initial precipitate, the magnetic properties are significantly deteriorated.
  • precipitation of compounds such as FeB and FeP in the soft magnetic powder can be suppressed, and the initial precipitate is basically bcc ⁇ Fe (—Si).
  • the volume ratio of the initial precipitate is not the volume ratio of the initial precipitate in each soft magnetic powder, but the volume ratio of the entire initial precipitate in the produced soft magnetic powder.
  • amorphous single-phase soft magnetic powder may be included, and the crystallinity 10% or more (3% or more) of soft magnetic powder may be included.
  • the particle size of the soft magnetic powder can be evaluated by a laser particle size distribution meter.
  • the average particle size of the soft magnetic powder can be calculated from the evaluated particle size.
  • the crystallinity and the particle size of the initial precipitate can be calculated by analyzing the measurement result by X-ray diffraction (XRD) by the WPPD method (Whole-powder-pattern decomposition method). From the peak position of the X-ray diffraction result, a precipitated phase such as an ⁇ Fe (—Si) phase or a compound phase can be identified.
  • the saturation magnetization and coercive force Hc of the soft magnetic powder can be measured using a vibrating sample magnetometer (VSM).
  • the saturation magnetic flux density Bs can be calculated from the measured saturation magnetization and density.
  • the Fe-based nanocrystalline alloy powder of this embodiment can be produced. More specifically, as described above, the soft magnetic powder of the present embodiment is subjected to heat treatment under a predetermined heat treatment condition, whereby bccFe nanocrystals are precipitated, and the Fe-based nanocrystal of the present embodiment is precipitated. Crystalline alloy powder is obtained.
  • This heat treatment needs to be performed at a temperature equal to or lower than the second crystallization start temperature (T x2 ) so as not to precipitate the compound phase. Specifically, the heat treatment in this embodiment needs to be performed at a temperature of 550 ° C. or lower. The heat treatment is preferably performed at a temperature of 300 ° C.
  • an inert atmosphere such as argon or nitrogen.
  • it may be partially heat-treated in an oxidizing atmosphere.
  • it may be partially heat-treated in a reducing atmosphere. Further, depending on the heat treatment conditions such as the temperature rising / falling rate and the holding temperature, a short time heat treatment at a higher temperature and a long time heat treatment at a lower temperature are possible.
  • the average particle size of the nanocrystals is preferably 50 nm or less, and more preferably 40 nm or less.
  • the crystallinity of the nanocrystal when the crystallinity of the nanocrystal is less than 25%, the saturation magnetic flux density Bs is slightly improved and the magnetostriction exceeds 20 ppm.
  • the crystallinity of the nanocrystal when the crystallinity of the nanocrystal is 40% or more, the saturation magnetic flux density Bs is improved to 1.6 T or more, and the magnetostriction is 15 ppm or less. Accordingly, the crystallinity of the nanocrystal is preferably 25% or more, and more preferably 40% or more.
  • the average particle size and crystallinity of the nanocrystals in the Fe-based nanocrystalline alloy powder can be measured and evaluated by XRD, as with the soft magnetic powder. Further, the saturation magnetic flux density Bs and the coercive force Hc of the Fe-based nanocrystalline alloy powder can be measured and calculated using VSM in the same manner as the soft magnetic powder.
  • the Fe-based nanocrystalline alloy powder according to the present embodiment can be molded to produce a magnetic part such as a magnetic sheet or a dust core. Moreover, magnetic parts, such as a transformer, an inductor, a reactor, a motor, and a generator, can be produced using the dust core.
  • the Fe-based nanocrystalline alloy powder of the present embodiment contains highly magnetized nanocrystals ( ⁇ cc of bccFe) at a high volume ratio. Further, the crystal magnetic anisotropy is low due to the refinement of ⁇ Fe. Moreover, magnetostriction is reduced by the mixed phase of the positive magnetostriction of the amorphous phase and the negative magnetostriction of the ⁇ Fe phase. For this reason, by using the Fe-based nanocrystalline alloy powder of the present embodiment, a dust core having a high saturation magnetic flux density Bs and a low core loss and excellent magnetic properties can be produced.
  • a magnetic part such as a magnetic sheet or a dust core by using soft magnetic powder before heat treatment instead of Fe-based nanocrystalline alloy powder.
  • a magnetic component or a dust core can be produced by forming a soft magnetic powder into a predetermined shape and then performing heat treatment under predetermined heat treatment conditions.
  • magnetic parts such as a transformer, an inductor, a reactor, a motor, and a generator, can be produced using the dust core.
  • the magnetic core manufacturing process of the dust core using the soft magnetic powder in the present embodiment will be described.
  • soft magnetic powder is mixed with a binder having good insulating properties such as resin and granulated to obtain granulated powder.
  • a binder having good insulating properties such as resin and granulated to obtain granulated powder.
  • a resin for example, silicone, epoxy, phenol, melamine, polyurethane, polyimide, or polyamideimide may be used.
  • phosphate, borate, chromate, oxide (silica, alumina, magnesia, etc.), inorganic polymer (polysilane) instead of or together with resin may be used as the binder.
  • Polygermane, polystannane, polysiloxane, polysilsesquioxane, polysilazane, polyborazirene, polyphosphazene, and the like may be used as the binder.
  • a plurality of binders may be used in combination, and a coating having a multilayer structure of two layers or more may be formed by different binders.
  • the amount of the binder is preferably about 0.1 to 10 mass%, and is preferably about 0.3 to 6 mass% in consideration of the insulation and the filling rate.
  • the amount of the binder may be appropriately determined in consideration of the powder particle size, application frequency, usage, and the like.
  • the granulated powder is then pressure-molded using a mold to obtain a green compact. Thereafter, the green compact is subjected to a heat treatment under a predetermined heat treatment condition, and nanocrystallization and a binder are cured simultaneously to obtain a dust core.
  • the pressure molding described above may be generally performed at room temperature.
  • pressure molding in a temperature range of 550 ° C. or less, extremely compact powder A magnetic core can also be formed.
  • the granulated powder when the granulated powder is pressure-molded, Fe, FeSi, FeSiCr, softer than the soft magnetic powder according to the present embodiment, in order to improve the filling property and suppress the heat generation in nanocrystallization.
  • You may mix powder, such as FeSiAl, FeNi, and carbonyl iron powder.
  • any soft magnetic powder having a particle diameter different from that of the soft magnetic powder according to the present embodiment may be mixed.
  • the mixing amount with respect to the soft magnetic powder according to the present embodiment is preferably 50 mass% or less.
  • the dust core in the present embodiment may be manufactured by a process different from the above-described magnetic core manufacturing process.
  • a dust core may be produced using the Fe-based nanocrystalline alloy powder according to the present embodiment.
  • the granulated powder may be produced in the same manner as the above-described magnetic core production process.
  • a powder magnetic core can be produced by pressure-molding the granulated powder using a mold.
  • the dust core of the present embodiment manufactured as described above includes the Fe-based nanocrystalline alloy powder of the present embodiment regardless of the manufacturing process.
  • the magnetic component of the present embodiment includes the Fe-based nanocrystalline alloy powder of the present embodiment.
  • Example 1 to 5 and Comparative Examples 1 to 8 Industrial pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were prepared as raw materials for the soft magnetic powders of Examples 1 to 5 and Comparative Examples 1 to 6 shown in Table 1 below.
  • the raw materials were weighed so as to have the alloy compositions of Examples 1 to 5 and Comparative Examples 1 to 6 shown in Table 1, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Thereafter, the molten alloy was processed by a water atomization method to produce an alloy powder (soft magnetic powder) having an average particle size of 32 to 48 ⁇ m.
  • the precipitated phase (precipitate) of the soft magnetic powder was evaluated by X-ray diffraction (XRD).
  • the soft magnetic powder was heat-treated in an argon atmosphere using an electric furnace under the heat treatment conditions shown in Table 1.
  • the saturation magnetic flux density Bs of the soft magnetic powder (Fe-based nanocrystalline alloy powder) after the heat treatment was measured using a vibrating sample magnetometer (VSM).
  • VSM vibrating sample magnetometer
  • a dust core was prepared from the soft magnetic powder before the heat treatment.
  • the soft magnetic powder was granulated using a 2 mass% silicone resin, and molded by a molding pressure of 10 ton / cm 2 using a mold having an outer diameter of 13 mm and an inner diameter of 8 mm, followed by a curing treatment.
  • the soft magnetic powders of Comparative Examples 1 to 4 contain 0.5 at% or more (0.4 at% or more) of Cu, and the core loss of the dust core is large. Further, the soft magnetic powders of Comparative Examples 5 and 6 do not contain Cu or contain less than 0.2 at% Cu, and the core loss of the dust core is large.
  • the soft magnetic powders of Examples 1 to 5 contain Cu in the range of 0.21 to 0.39 at%, and the core loss of the dust core is higher than that of the dust core of Comparative Example 7. Are better.
  • the soft magnetic powders of Examples 1 to 3 contain Cu in the range of 0.31 to 0.39 at%, and the core loss of the dust core is higher than that of the dust core of Comparative Example 8. Are better.
  • the soft magnetic powder (Fe-based nanocrystalline alloy powder) after heat treatment in Examples 1 and 2 has a high saturation magnetic flux density Bs of 1.7 T or more. From the above measurement results, it can be understood that the ratio of Cu contained in the soft magnetic powder is preferably 0.2 at% or more and less than 0.4 at%. Moreover, it can be understood from the comparison between Example 5 and Comparative Example 5 that the average particle size of the nanocrystals in the Fe-based nanocrystal alloy powder is preferably 50 nm or less.
  • Example 6 to 13 and Comparative Examples 9 to 14 Industrial pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were prepared as raw materials for soft magnetic powders of Examples 6 to 13 and Comparative Examples 9 to 12 shown in Tables 2 and 3 below.
  • the raw materials were weighed so as to have the alloy compositions of Examples 6 to 13 and Comparative Examples 9 to 12 shown in Tables 2 and 3, and melted by high frequency melting in an argon atmosphere to prepare molten alloys. Thereafter, the molten alloy was processed by a water atomization method to produce an alloy powder (soft magnetic powder). Thereafter, the soft magnetic powders were classified to produce a plurality of types of soft magnetic powders having the average particle sizes shown in Table 2.
  • the precipitated phase (precipitate) and crystallinity of the soft magnetic powder after classification were evaluated by XRD. Further, the classified soft magnetic powder was subjected to a heat treatment in an argon atmosphere under the heat treatment conditions shown in Table 2 using an electric furnace. The coercive force Hc and the saturation magnetic flux density Bs of the soft magnetic powder (Fe-based nanocrystalline alloy powder) after the heat treatment were measured using VSM. The average particle size of the nanocrystals in the Fe-based nanocrystal alloy powder was measured and evaluated by XRD. A dust core was prepared from the soft magnetic powder after classification and before heat treatment.
  • the soft magnetic powder was granulated using a 2 mass% silicone resin, and molded by a molding pressure of 10 ton / cm 2 using a mold having an outer diameter of 13 mm and an inner diameter of 8 mm, followed by a curing treatment. Thereafter, using an electric furnace, heat treatment was performed in an argon atmosphere under the heat treatment conditions shown in Table 2, and a dust core was produced. Using an AC BH analyzer, the core loss of 20 kHz-100 mT was measured for the dust core. As Comparative Examples 13 and 14, dust cores were prepared using soft magnetic powders of FeSiCr and Fe amorphous (FeSiB), and measured in the same manner as the dust cores of Examples 6 to 13 and Comparative Examples 9 to 12. And evaluated. The results of the above measurement and evaluation are shown in Table 2 and Table 3.
  • the soft magnetic powders of Comparative Examples 9 to 12 have a crystallinity higher than 10%. For this reason, even if heat treatment for nanocrystallization is performed, both the coercive force Hc of the soft magnetic powder (Fe-based nanocrystal alloy powder) after heat treatment and the core loss of the dust core are remarkably large. In particular, the magnetic properties of the Fe-based nanocrystalline alloy powders and dust cores of Comparative Examples 10 to 12 in which the compound phase is precipitated are significantly deteriorated.
  • the soft magnetic powders of Examples 6 to 13 have a crystallinity of 10% or less, and have a saturation magnetic flux density Bs higher than that of the Fe-based nanocrystalline alloy powders of Comparative Examples 13 and 14 by heat treatment. Furthermore, the coercive force Hc of the Fe-based nanocrystalline alloy powders in Examples 6 to 13 and the core loss of the dust core are superior to those of the dust core of Comparative Example 13. In particular, the soft magnetic powders of Examples 6 to 8 and 10 to 12 have a low crystallinity of 3% or less. For this reason, the soft magnetic powders and dust cores of Examples 6 to 8 and 10 to 12 have magnetic characteristics superior to those of the dust core of Comparative Example 14 when heat-treated.
  • Examples 14 to 21 and Comparative Examples 15 to 20 Industrial pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were prepared as raw materials for the soft magnetic powders of Examples 14 to 21 and Comparative Examples 15 to 18 shown in Tables 4 and 5 below.
  • the raw materials were weighed so as to have the alloy compositions of Examples 14 to 21 and Comparative Examples 15 to 18 shown in Table 4 and Table 5, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Thereafter, the molten alloy was processed by a water atomization method to produce an alloy powder (soft magnetic powder) having an average particle size of 36 to 49 ⁇ m.
  • the precipitated phase (precipitate) and crystallinity of the soft magnetic powder were evaluated by XRD, and the saturation magnetic flux density Bs of the soft magnetic powder was measured using VSM. Further, the soft magnetic powder was heat-treated in an argon atmosphere using an electric furnace under the heat treatment conditions shown in Table 5. The saturation magnetic flux density Bs of the soft magnetic powder (Fe-based nanocrystalline alloy powder) after the heat treatment was measured using VSM. In addition to the preparation of the Fe-based nanocrystalline alloy powder, a dust core was prepared from the soft magnetic powder before the heat treatment.
  • the soft magnetic powder was granulated using a 2 mass% silicone resin, and molded by a molding pressure of 10 ton / cm 2 using a mold having an outer diameter of 13 mm and an inner diameter of 8 mm, followed by a curing treatment. Thereafter, using an electric furnace, heat treatment was performed in an argon atmosphere under the heat treatment conditions shown in Table 5 to produce a dust core. Using an AC BH analyzer, the core loss of 20 kHz-100 mT was measured for the dust core. Further, as Comparative Examples 19 and 20, dust cores were prepared using FeSiCr and Fe amorphous (FeSiB) soft magnetic powders, and the same as the dust cores of Examples 14 to 21 and Comparative Examples 15 to 18. Measured and evaluated. The results of the above measurement and evaluation are shown in Table 4 and Table 5.
  • the composition range of the soft magnetic powders of Comparative Examples 15 to 18 is outside the scope of the present invention, and the saturation of the soft magnetic powder (Fe-based nanocrystalline alloy powder) after the heat treatment
  • the magnetic flux density Bs is low, or the core loss of the dust core is inferior to that of the dust cores of Comparative Examples 19 and 20.
  • the composition range of the soft magnetic powders of Examples 14 to 21 is within the range of the present invention, and by suppressing the crystallinity to 10% or less, the magnetic properties after the heat treatment are improved, and the crystallinity is 3%. By suppressing to the following, the magnetic properties after the heat treatment are further improved.
  • the Fe ratio is 79 at% or more and 84.5 at% or less, and the Si ratio is less than 6 at% (including zero).
  • the ratio of B is preferably 4 at% or more and 10 at% or less, the ratio of P is greater than 4 at% and 11 at% or less, and the ratio of Cu is preferably 0.2 at% or more and less than 0.4 at%.
  • the proportion of Fe should be 83.5 at% or less, the proportion of B should be 8.5 at% or less, and the proportion of P should be 5.5 at% or more. preferable.
  • the ratio of P is 8 at% or less.
  • Examples 22 to 30 As raw materials for the soft magnetic powders of Examples 22 to 30 shown in Tables 6 and 7 below, industrial pure iron, ferrosilicon, ferroline, ferroboron, electrolytic copper, ferrochrome, carbon, niobium, molybdenum, Co, Ni, tin , Zinc, and Mn were prepared. The raw materials were weighed so as to have the alloy compositions of Examples 22 to 30 described in Tables 6 and 7, and melted by high frequency melting in an argon atmosphere to prepare molten alloys. Thereafter, the molten alloy was processed by a water atomization method to produce an alloy powder (soft magnetic powder) having an average particle size of 32 to 48 ⁇ m.
  • Examples 31 to 48 As raw materials for the soft magnetic powders of Examples 31 to 48 described in Table 8 and Table 9 below, industrial pure iron, ferrosilicon, ferroline, ferroboron, electrolytic copper, carbon, ferrochrome, Mn, Al, Ti, and FeS Prepared. The raw materials were weighed so as to have the alloy compositions of Examples 31 to 48 shown in Table 8, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Thereafter, the molten alloy was processed by a water atomization method to produce an alloy powder (soft magnetic powder) having an average particle size of 35 ⁇ m. The precipitated phases (precipitates) and crystallinity of the soft magnetic powders in Examples 31 to 48 were evaluated by XRD.
  • the soft magnetic powder was heat-treated in an argon atmosphere using an electric furnace under the heat treatment conditions shown in Table 9.
  • the saturation magnetic flux density Bs of the soft magnetic powder (Fe-based nanocrystalline alloy powder) after the heat treatment was measured using VSM.
  • a dust core was prepared from the soft magnetic powder before the heat treatment.
  • the soft magnetic powder was granulated using a 2 mass% silicone resin, and molded by a molding pressure of 10 ton / cm 2 using a mold having an outer diameter of 13 mm and an inner diameter of 8 mm, followed by a curing treatment. Thereafter, using an electric furnace, heat treatment was performed in an argon atmosphere under the heat treatment conditions described in Table 9 to produce a dust core.
  • the core loss of 20 kHz-100 mT was measured for the dust core. Table 9 shows the results of the above measurement and evaluation.
  • Examples 31 to 48 contain Al, Ti, S, O, and N as trace elements in various contents.
  • the compositions of Fe, Si, B, P and Cu are the same.
  • the crystallinity of Examples 31 to 48 is as low as 10% or less, and the saturation magnetic flux density Bs of Examples 31 to 48 is as good as 1.63 T or more.
  • the core loss of Examples 31 to 48 is also good at 220 kW / m 3 or less.
  • the Al content increases, the crystallinity and core loss increase, and the saturation magnetic flux density Bs decreases.
  • the Al content is preferably 0.1% by mass or less, and 0.01% by mass or less from the viewpoint of greatly reducing the core loss. Is more preferable.
  • the Ti content is preferably 0.1% by mass or less, and 0.01% by mass or less from the viewpoint of greatly reducing the core loss. Is more preferable.
  • the S content increases, the crystallinity and core loss increase, and the saturation magnetic flux density Bs decreases.
  • the S content is preferably 0.1% by mass or less, and 0.05% by mass or less from the viewpoint of greatly reducing the core loss. Is more preferable.
  • the core loss increases as the O content increases.
  • the content of O is preferably 1% by mass or less, and more preferably 0.3% by mass or less, from the viewpoint of reducing core loss.
  • the N content is preferably 0.01% by mass or less, and more preferably 0.002% by mass or less, from the viewpoint of reducing crystallinity and core loss.
  • Examples 49 to 53 Industrial pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were prepared as raw materials for the soft magnetic powders of Examples 49 to 53 shown in Tables 10 and 11 below.
  • the raw materials were weighed so as to have the alloy compositions of Examples 49 to 53 described in Table 10 and Table 11, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Thereafter, the molten alloy was processed by a water atomization method to produce an alloy powder (soft magnetic powder) having an average particle size of 40 ⁇ m.
  • the precipitated phases (precipitates) and crystallinity of the soft magnetic powders in Examples 49 to 53 were evaluated by XRD.
  • the soft magnetic powder was heat-treated in an argon atmosphere using an electric furnace under the heat treatment conditions shown in Table 10.
  • the saturation magnetic flux density Bs of the soft magnetic powder (Fe-based nanocrystalline alloy powder) after the heat treatment was measured using VSM.
  • a dust core was prepared from the soft magnetic powder before the heat treatment.
  • the soft magnetic powder was granulated using a 2 mass% silicone resin, and molded by a molding pressure of 10 ton / cm 2 using a mold having an outer diameter of 13 mm and an inner diameter of 8 mm, followed by a curing treatment. Thereafter, using an electric furnace, heat treatment was performed in an argon atmosphere under the heat treatment conditions shown in Table 10 to produce a dust core.
  • Example 49 slight corrosion was confirmed after the constant temperature and humidity test, but in Examples 50 to 53, it can be seen that the corrosion situation was improved. From this result, it can be seen that the ratio of P in the soft magnetic powder is preferably larger than 5 at%.
  • the soft magnetic powders of Examples 49 and 50 have a crystallinity of greater than 3%, while the soft magnetic powders of Examples 51 to 53 have a low crystallinity of 3% or less.
  • the core loss of the dust cores of Examples 51 to 53 is lower than that of the dust cores of Examples 49 and 50.
  • the proportion of Fe is 83.5 at% or less
  • the proportion of B is 8.5 at% or less
  • the proportion of P is 5. It turns out that it is preferable that it is 5 at% or more. Further, referring to Examples 52 and 53, it can be seen that the core loss of the dust core can be reduced by setting the ratio of P in the soft magnetic powder to 6 at% or more.
  • the present invention is based on Japanese Patent Application No. 2017-012977 filed with the Japan Patent Office on January 27, 2017, the contents of which are incorporated herein by reference.

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Abstract

L'invention porte sur une poudre magnétique à aimantation temporaire représentée par la formule générale FeaSibBcPdCueà l'exception des impuretés inévitables. Dans la formule de la composition, a, b, c, d et e sont tels que 79 ≤ a ≤ 84,5 en %, 0 ≤ b {t; 6 en %, 4 ≤ c ≤ 10 en %, 4 {t; d ≤ 11 en %, 0,2 ≤ e {t; 0,4 en %, et a + b + c + d + e = 100 en %.
PCT/JP2018/002380 2017-01-27 2018-01-26 POUDRE MAGNÉTIQUE À AIMANTATION PROVISOIRE, POUDRE D'ALLIAGE NANOCRISTALLIN À BASE DE Fe, COMPOSANT MAGNÉTIQUE ET NOYAU DE POUSSIÈRE Ceased WO2018139563A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
US16/481,449 US11814707B2 (en) 2017-01-27 2018-01-26 Soft magnetic powder, Fe-based nanocrystalline alloy powder, magnetic component and dust core
SE1950904A SE543592C2 (en) 2017-01-27 2018-01-26 SOFT MAGNETIC POWDER, Fe-BASED NANOCRYSTALLINE ALLOY POWDER, MAGNETIC COMPONENT AND DUST CORE
CA3051184A CA3051184C (fr) 2017-01-27 2018-01-26 Poudre magnetique a aimantation provisoire, poudre d'alliage nanocristallin a base de fe, composant magnetique et noyau de poussiere
JP2018552901A JP6472939B2 (ja) 2017-01-27 2018-01-26 軟磁性粉末、Ｆｅ基ナノ結晶合金粉末、磁性部品及び圧粉磁芯
CN201880008431.9A CN110225801B (zh) 2017-01-27 2018-01-26 软磁性粉末、Fe基纳米晶合金粉末、磁性部件及压粉磁芯
KR1020197021757A KR102259446B1 (ko) 2017-01-27 2018-01-26 연자성 분말, Fe 기 나노 결정 합금 분말, 자성 부품 및 압분 자심

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Cited By (5)

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WO2020026949A1 (fr) * 2018-07-31 2020-02-06 Ｊｆｅスチール株式会社 Poudre magnétique à aimantation douce, poudre d'alliage nanocristallin à base de fer, composant magnétique et noyau à poudre
JP2020147765A (ja) * 2019-03-11 2020-09-17 Tdk株式会社 軟磁性合金および磁性部品
JPWO2021132272A1 (fr) * 2019-12-25 2021-07-01
WO2021149590A1 (fr) * 2020-01-23 2021-07-29 株式会社東北マグネットインスティテュート Alliage et corps moulé
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US11814707B2 (en) 2023-11-14
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CA3051184C (fr) 2022-04-05
US20190362871A1 (en) 2019-11-28
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CN110225801A (zh) 2019-09-10
CN110225801B (zh) 2022-01-18

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